I organized by Sathyabama University, Chennai, India in association with DRDO, New Delhi, India, 24th _26tl" July, 2013

AiClJ Proceedings of the "International Conference on Advanced Nanomaterials & Emerging Engineering Technologies" (ICANMEET-20J3)
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A Review on the Use ofNanoindentation Technique

in Characterizing Cement-Based Materials
#1 #2
Salim Barbhuiya , Hamid Nikraz
# Department of Civil Engineering

Curtin University a/Technology, Perth, Australia

'Salim.Barbhuiya@curtin.edu.au
'H.Nikraz@curtin.edu.au
Abstract-In this paper an attempt has been made to provide The hardness of materials could also be measured by other
an overview on the use of nanoindentation technique in methods based on a similar underlying principle. One of these
characterizing cement-based materials. The basic principle of alternative methods was the one suggested by George E.
nanoindentation is described. The mathematical formulation to
Sandland and Robert L. Smith in 1921 at Vickers Ltd. This
determine the mechanical properties fro nanoindentation is
test was not only easier to use than the existing tests but also
vividly discussed. A discussion is also made on the nano
had the advantage that the required calculations were not
mechanical properties of different phases in cement paste.
Finally, the challenges in using the nanoindentation technique in affected by size of the indenter used in performing the test.
characterizing cement-based materials are highlighted. Another advantage lay in the fact that the same indenter could
Kwords-nanoindentation, cement-based materials, caIcium be used for all materials with no consideration of hardness of
silicate-hydrate gel, young's modulus, hardness the specimen to be tested being taken into account. On
application of loads on the indenter, every material offers
I. INTRODUCTION some resistance against plastic deformation and the
Localised contact response measured by instrumental measurement of this resistance is the underlying principle of
indentation has long been used to characterize material the Vickers test. The resistance offered by each specimen is
mechanical properties along with other conventional and still expressed in terms of a standard thus enabling comparison of
widely used methods like uniaxial compression and tension, specimen materials-the Vickers Pyramid Number (HV) or
unconfmed compression and tension etc. Such an approach Diamond Pyramid Hardness (DPH). The hardness number has
provides a continuous record of variation in depth of the units of pascals. However, HV and DPH do not represent
penetration as a function of load imposed into indented pressure in any way as they are obtained by dividing load
specimen surface [I]. The application of such methods goes applied with the area of the indent made and not the area
right back to 1900.The Brinell hardness test along with the perpendicular to direction of application of force. Basic
hardness number/scale was proposed by the Swedish requirements governing choice of indenter to be used in the
engineer Johan August Brinell. As a part of the test, specimen Vickers test are that impressions made on specimens should
was indented with a ball made of hardened steel or carbide, 10 have similar geometry and this should not depend on the size
mm in diameter. A load of 3000 kg was imposed on the ball of the indenter. Presence of points whose position could be
commonly in tests. Excessive indentation was avoided in case measured to a high accuracy was also necessary. Moreover the
of softer materials by reducing the imposed load to 1500 kg or indenter should have sufficient resistance against getting
500 kg. For iron and steel specimens the full load is applied deformed under the applied load. An indenter having the
for a period of 10-15 seconds. This period may widely vary shape of square-based pyramid is commonly used. Choice of
for other materials and full loads may have to be applied for material for the indenter is commonly diamond. They both
periods up to 30 seconds. The size of the indentation was satisfy almost all requirements and fulfill the assumptions
measured using low power microscopy techniques. Materials made while calculating formulae used in the Vickers Test [3].
possessing heterogeneous structures are commonly tested for
Formulae used in calculation of HVIDPH are:
hardness using the Brinell hardness test [2].Page Layout
An easy way to comply with the conference paper d2
A=
2 sin(136' /2)
------
formatting requirements is to use this document as a template
and simply type your text into it.
d2
A=
1.8544
Brinell hardness number, --

''
BHN= -----------

"- /)(1) - /)2 _ /)2 )
F 1.8544F
HV = =
2 ' A d2
where
where
D is the used indenter's diameter
A :surface area of indentation (mm2)
D; is the size or diameter of the indentation made F :applied load on indenter (kgf)

d :length of diagonal left in indention (mm)

978-1-4799-1379-4/13/$31.002013 IEEE 613

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Other indentation hardness tests include the Rockwell technologies or other powerful techniques like atomic force
Indentation Test Principle patented in [9 [4.The underlying microscopy, scanning electron microscopy. Indenters used are
principle of the Rockwell Indentation Test-differential depth also those which have their geometries known to very high
hardness measurement concept was first proposed by precision and this also helps to overcome a lot of problems
Viennese scientist Paul Ludwik. Unlike existing hardness faced in determining contact geometry [6].
measurement tests this test does not involve measurement of
the size of the indentation left by the indenter in the specimen [I. PR[NC[PLE OF NANO[NDENTAT[ON

upon application of load on the indenter but rather involves
measurement of the difference in the depth up to which the
indenter penetrates under two different loads or at different
times during the loading cycle applied. At first a minor load is
applied on the indenter and the depth of penetration is noted.
The minor load is followed by a major load and another
subsequent measurement of penetration depth under that load.
[t is the difference in penetration depth under the minor and
major loads that is crucial for measuring the Rockwell
hardness of a specimen. This method scores above other
methods simply in the fact that while
measuring methods involve lot of cumbersome calculations
this method avoids a lot of them and makes
measurement relatively fast, easy and simple [4].
The first method of measuring mechanical properties of
materials at a micro scale was the Knoop indentation test.
Specimens, which allow only small indentations to be made in
them, like brittle materials or sheets with very less thickness
could be measured for hardness very effectively by the Knoop
indentation test. Shape of the indenter used is pyramidal.
Choice of material for the indenter preferred is diamond. A
load is applied on this indenter for a specific time period. The
indentation left behind is then examined and its size is
measured with the help of a microscope. Formulae giving the
value of Knoop hardness HK or KHN are [5] shown below:
The basic principle of Nanoindentation is that a prescribed
load is applied to an indenter (usually of known geometry) in
contact with the specimen/material to be tested. With
increased load the depth of penetration is measured to obtain a
continuous record of penetration with loading. The loading is
increased on the indenter till the penetration reaches a user
defined value and thereafter the load might be either kept
constant or removed. The contact area between the indenter
and the material being tested is determined by knowing the
penetration depth of the indenter at full loading and then
other hardness deriving it from the geometry of the indenter or by light
microscopy. Value of Hardness of the specimen is calculated
hardness by measurement of the quantities of applied load and also the
area of contact-
Hardness,
where
H refers to hardness of the indented material
Pmax refers to maximum load on indenter
Ar refers to residual indention area
A measure of modulus of elasticity of the specimen being

HK=
load(kgf) P tested is obtained from the nature of the P-h plot during
impression area _

unloading

where L is the length of the indentation along the axis

about which its length is aligned, Cp factor introduced to

account for the shape of the used indenter. In ideal cases it is

taken as .070279 P load applied on the indenter to produce the
indentation in the specimen
Despite the long usage of indentation methods in
determining material properties, very little information is
known and not much research has been done in characterizing
cement based materials at the nano scale and correlating these
11M
properties with overall properties like strength, ductility,
durability etc. [n a large sense, Nanoindendation in a larger
meaning is the name given to a large group of indentation
Fig I. Load-displacement curve for instrumented indentation [7]
tests. In these indentation tests indentation is performed on
specimens of small volumes using very small loads and III MATHEMATICAL FORMULATION TO
indenters, which are even smaller, the specimens being tested. DETERM[NE MECHAN[CAL PROPERT[ES FROM
Both the volume of the specimen and the size of the indenter NANOINDENTAnON
being small, it is only natural that the contact area of the
Data collected when nanoindentation tests are performed
indenter and the specimen cannot be easily found and this
are most commonly in terms of corresponding values of load
poses as a major challenge while finding the hardness during
on the indenter and the depth of the specimen to which the
nanoindentation tests. These problems are however overcome
by coupling nanoindentation with advanced imaging indenter penetrates under that given load. A P-h plot is

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plotted from such observations. Values of modulus of TABLE I:

elasticity and penetration resistance/hardness are calculated COMMONLY USED INDENTERS
from this curve by various mathematical formulations, which mvE NTLK ,'KU,'"L '"V 'lli,uANULL """LUn m'"KLU' \.J (hVl.t. TK :
rYPI' ARI;i\ CONI': ANG),]'; ).'i\CTOR CORRITTION
will be discussed in this section. The analysis is based on the 8 (DEGREE) FACTOR

(Al a
stress distribution problems solved by Boussinesq and Hertz. (DEGREE)
0:\)

7r2Rhp
Hertz obtained relationships between the radius of the area in Sphere NlA NlA o. )
contact between the specimen and the indenter, the load which
was being applied on indenter for the corresponding
llt:r\..:ovich
3,fih tan2 () (,5.l 70,2')')(, 0,75 LOJ4

considered contact area and depth of penetration, size of the

indenter and elastic properties of both the indenter and the Vickers
4h2tan2(}
I'
(,< 70_32 0,75 1.012

specimen as: Knoop

2hl tan e. tan e, -86.25 77.(4 0,75 1.012

3 3PR 0,75 1.012

a =-- 8],-65
4,
Cube Corner
3,fihl tan2 () ::'),_6 4 ._ o. ) 1.034

Where, a: radius of the area in contact between the indenter

and the specimen being tested, R : indenter radius, P : load on 7rh tan' IX IX IX 0.7_

indente Er : Reduced modulus/indentation modulus/combined

modulus, A Factor representing elastic properties of both

indenter and specimen. It is calculated as:

I l-v2 1-1/'2
-=--+---
Er E E'

E',
'
Where, v Modulus of elasticity and Poisson's ratio of the
specimen, E, V Modulus of elasticity and Poisson's ratio of Fig 2, Commonly used indenters
the indenter, The depth of penetration hi and load on indenter
being tested by indentation.
A: Area projected by the region, which suffers indentation
are related as:
when a load is applied on the indenter
Though originally the calculations where done considering
a conical indenter, this equation can be used to obtain results
to the same degree of accuracy as with conical indenters for
For the case of Conical indenters, the relationship between
indentations performed with other indenters too (spherical and
load applied on the indenter for penetration into the sample
cylindrical).
and the radius of the area of contact between the indenter and
specimen was obtained as:

1W P
P=-E acota
2 r
SURFACE PROFILE AFTER
LOAD RaKlYAl
I
Where, a: cone semi angle, a cot a : corresponding depth of
,
indentation, Thus,

2Etana h2
P= I
1r

Commonly used indenters with contact area between the

indenter and material being indented given as a function of
depth of the indentation left behind by the indenter are given
in Table 1 and Fig. 2 Instrumented microhardness was
introduced popularly by Buylchev, Alekhin, Shorshorov who
analysed their findings with the equation they themselves
Fig 3, Schematic representation of a section through an indenter [8]
proposed: A. Oliver and Pharr method
dP
s
dH
Suggested in 1992, the Oliver and Pharr method presents an
analytical solution of the nanoindentation problem. Shape
where
functions of indenters are calculated and these are used to give
s = dP
values of the area in contact between the indenter and the
dH
specimen during nanoindentation from the depth of the
gives us a measure of stiffness of the specimen indented area. This method is known as depth-sensing

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indentation testing [8]. The total displacement h can be The Cheng and Cheng'S formula when maximum load

expressed as the sum of two separate quantities according to applied nax is bought in reduces to:
the Oliver and Pharr method:

h =he +h,
i Pmax _
H
Jr
S2 M2
where

he Distance along the vertical direction in the direction

Here, ()I ' l ' "ax can be obtained from the P - h graph

corresponding to the nanoindentation experiment. This

contact is occurring or the contact depth
method presents a unique approach via which the hardness as
h, Displacement of the surface at the contact perimeter well as indentation modulus can be calculated without
Let us consider a situation when load applied on the calculation of contact area.
C. Duel Indentation Technique
indenter is the peak load Pmax and when radius of area in
This method involves the indentation of the specimen with
contact, which is circular, has a value a two different indenters (having two different geometries).

( )
The displacement under these conditions is also maximum Contact Area is then expressed as-
hmax . Final depth of the indentation after the 2
and has a value Jr
sexp(i)
indenter has been fully withdrawn is hf. The projected area
AcU) =- --
4 M
A is expressed from a functional relationship of contact depth where
he as: i =1, 2 for first and second indenter respectively
A=F(hJ Sexp stiffness

The functional relationship is defined by performing pexp load on indenter

analysis on a material of known indentation modulus prior to hexp maximum depth of indentation
performing analysis on the specimen. All the above-mentioned quantities should correspond to
Now from Fig. 3, we get
value of i particular indenter.
he =hmax -h, Since M is same in both the experiments, the ratio of
For conical indenters:

h, = (tr - 2) (h
tr
_ h J. )
and
(h - h J. ) = 2
S
hardness from both the experiments is-

H(l)
=
pexp(l) x( sexp(1) y
)
Thus we have: H(2). pexp(2). sexp(2)
Pm ax
hs =E Contact areas are then calculated using any method and the
S
values of hardness and modulus are estimated using-
where
2
pexp(i) sexp(i)
2
Hest(i) =---. and M
esl(i)
J7i A:sIU)
-(Ji' - 2) 0.72 = ----===
A:SI(l)
E = =
Ji'
B. Cheng and Cheng's Method
Cheng and Cheng performed a large number of indentation Iterations are done till we get M
e"I(I) = Me,,1(2) = Mexp(l)
experiments through finite element simulation. These
simulations were performed on a large number of materials, IV NANO-MECHANICAL PROPERTIES OF
which show different behaviour of strain hardening. These DIFFERENT PHASES IN CEMENT PASTE
formulae were arrived at while in fact analysing the The main phases present in the microstructure of cement
accumulation of material that takes place around the based materials are:
indentation during nanoindentation. A relationship was found
I. Calcium Silicate Hydrate, C-S-H
to exist between hardness of the specimen, the reduced
modulus of the indenter and the specimen, work done during
2. Calcium Hydroxide, CH
3. Ettringite
loading and work done during unloading of the indenter (both

P -h
4. Monosulfate
calculated from plot). This relationship is expressed as
5. Unhydrated cement particle
[9-13]:
6. Air voids
()I - l
",0:1-5 H
The heterogeneous nature of concrete can be observed at

()I M scales ranging from macro to micro as shown in Fig. 2.

Fundamental properties of concrete like strength, ductility,
where
creep and shrinkage are closely related to the microstructure
Ol area under loading curve of concrete (especially the Calcium Silicate Hydrate phases).
An in-depth knowledge of the constituent structure of concrete
l
area under unloading curve
at the nano scale and its relationship with the mechanical

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properties will allow control of the above mentioned 4. Fourth type: [t forms during later stages of hydration.
macroscopic properties from the nano-scale itself. Morphologically it also has a massive structure similar to
Development of nano-engineered materials also requires a the third type. Absence of features in the morphology is
detailed knowledge of the microstructure and resulting also to be noted.
changes in it on addition of modifiers, Such knowledge might
Scanning electron microscopy however provides
be the answer to the industry's need for high-performance,
information, which is not representative of the bulk
durable, and sustainable construction materials and offers an
microstructure because of dehydration of the sample, which
opportunity to transform concrete into something way more
occurs due to exposure to high vacuum in some stages of
robust and environmentally sustainable material than its
scanning electron microscopy. Experiments with the help of
present commercially available forms.
light microscopy, TEM and X ray mapping, Neutron
Scattering however suggested the presence of two
morphologically distinct forms of Calcium Silicate Hydrate
= +
"----,- ---...... Anrt' Cement Paste Sand
which are referred to as:

[. Phenograins - Groundmass,or
2. Outer product - Inner product, or
3. Low density - High density, or
4. Middle product - Late product.
Moreover a number of models of C-S-H were developed to
give both quantitative and qualitative information. Both forms
of Calcium Silicate Hydrate were considered in the model
proposed by Jennings and Tennis [16-18]. The results
proposed by using scanning electron microscopy by Diamond
[15] were found to be consistent with the model proposed.
Fig.2. Concrete at different length scales [14] Experiments were performed in which nitrogen sorption by

CSH (Calcium Silicate Hydrate) gel forms the most the phases was measured. A few of the pores of Low Density

important phase in the microstructure of concrete. This phase Calcium Silicate Hydrate are assumed to be accessible to

forms the principal binding material in concrete. A definite nitrogen. On the other hand none of the pores of High Density

chemical structure or composition cannot be attributed to CSH Calcium Silicate Hydrate are accessible to nitrogen. Thus

in concrete and it exists as a poor crystal. Calcium Silicate values of surface area, which undergo nitrogen sorption as put

Hydrate is the primary product of hydration in cementious forward by this study, correspond only to regions where the

materials. [t is also the phase that has the highest volume low-density phase is present. [t is postulated that the same unit

fraction in such materials sometimes accounting up to 70% of builds up both the phases. This unit-the globule is same for

the total volume. Thus it is seen that it is this phase, which both the forms of Calcium Silicate Hydrate but only occurs in

contributes the most to the mechanical properties of concrete. different packing efficiencies in the two forms i.e. with

In the scale of nanometres, Calcium Silicate Hydrate Gel is packing density of 0.63 in Low Density Calcium Silicate

seen to possess a pore structure with pores having dimensions Hydrate and 0.76 in High Density Calcium Silicate Hydrate.

of several nanometres, a structure similar to that possessed by The packing density in High Density Calcium Silicate Hydrate

colloidal gels. As a result the surface area of the interface is close to the densest packing density for spheres arranged in

between the solid phase and liquid phase present in concrete a crystalline order in a lattice. The presence of two types of

becomes very large. It is this fact, which causes concrete to calcium silicate hydrate is confirmed by results obtained from

behave like a poro-visco-elastic material. This nature of nanoindentation tests performed on intact and calcium leached

concrete is evident in its reaction to both mechanical loading materials. These tests also confirm their role in elastic

and drying. stiffness and hardness of cement based materials.

Diamond [15] classified Calcium Silicate Hydrate Gels into Macro properties of cementious materials like hardness,

four forms based on their morphology using scanning electron strength, ductility etc have been established to have direct and

microscopy: indirect relationships with the nano-mechanical characteristics

l. First type: It is an early product. Has the morphology of of cementious materials obtained via nanoindentation and

long fibre other techniques. A lot of such research has been performed
by treating cement-based materials as a continuous bulk
2. Second type: It forms in early stages of hydration. Has a medium. Nanomechanical properties of different phases of
structure similar to that of honeycombs and reticular cement based materials not only provide valuable input into
networks development of microstructural modelling of concrete but also
help in understanding data obtained from other studies of
3. Third type: Occurs in higher fractions in older mixes.
mechanical properties of such materials especially those
Morphologically has a massive structure and has higher
which treat the materials as a continuous bulk medium.
density
Moreover, these properties have been successfully related to

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spatial features, especially across the Interfacial Transition
Zone.
V CHALLENGES IN USING NANOINDENTATION
TECHNIQUE IN CHARACTERISING CEMENT-BASED
MATERIALS
Modelling of mechanical properties of materials at all
scales forms an integral part of research in cementious
materials and nanoindentation can arguably be credited to be
responsible for quite a few major breakthroughs in this field.
However, a few challenges still arise when Nanoindentation is
used to characterize cement-based materials even now. A
common challenge faced in nanoindentation is preparation of
the sample surface. The theory behind nanoindentation makes
it applicable only to completely flat surfaces but it is seen that
samples of cement based materials have unaffected surface
roughness in the scale of hundreds of nanometres, almost of
the same scale to which indentations are made. This however
maybe worked upon by polishing though natural porosity of
cement itself results in roughness in the order of hundreds of
nanometres. Thus surface roughness of sample suggests that
indentation depth be in the scale of 1flm [19- 21].
The procedure of calculating hardness and elastic modulus
is applicable strictly for homogenous materials whereas all
cement-based materials tend to be heterogeneous at all scales
including the nano-scale. A statistical approach through the
grid/statistical nanoindentation method has been formulated to
overcome or offset the requirement for homogeneity of the
specimen. A large number of positions are selected for making
indents with the objective of obtaining a representative sample
area and results, which can be then interpreted statistically.
However a more accurate method might be to select points for
making indents manually rather than randomly in a way such
that they correspond to a certain phase and
mechanical properties corresponding to that phase can be
obtained directly. It is seen that in a cement paste homogenous
3
products exist in volumes of 2flm or larger. This suggests that
indentation depth be in the scale of 150-200nm in order to
obtain a satisfactory statistical distribution [22].
The aforementioned conditions both suggest limits on the
indentation depths, which contradict each other. Possible
solutions to this include using samples, which are artificial
systems with reduced porosity, surface roughness or having
larger volumes of homogenous phases. However, it cannot be
said with absolute confidence that mechanical properties of
phases in such artificial systems will represent mechanical
properties of cement-based materials accurately. Moreover in
compliance with grid/statistical nanoindentation, if the size of
proposed nanogranular globuli of the specimen material is
known then the indentation depth should be chosen in such a
way so that it is larger than the nanogranular globuli and at the
same time smaller than average size of region that can be
considered homogenous. However indentation
employed sometimes also fail these criteria [23- 25].
m
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associatIOn wIth DRDO, New Deihl, IndIa, 24 -26 , July, 2013
VI CONCLUDING REMARKS
Nanoindentation makes accessible a scale where physical
chemistry meets mechanics and is probably one of the only
existing methods that can do so. Thus it can be evaluated as
a highly effective method of characterization of cement based
materials. Nanoindentation involves an approach which
models these materials as chemically stable equilibrium thus
enabling the resolution and expression of relationships of
properties which can be studied at the macro level in terms of
properties of components at the nano scale which change
neither with time and are invariably are present in all such
materials. Curing age, water to cement ratio, micro- and nano
modifiers and other parameters which govern the nature of
cementious materials-whether these factors have some sort of
impact on the nano-mechanical properties of such materials is
something which can be effectively studied only with an
approach which involves nanoindentation in some scale.
Findings from nanoindentation can help not only control
fundamental properties of such materials but also engineer
new materials with improved properties. However, certain
shortcomings and challenges do arise when trying to use this
method to characterize cement-based materials. The accuracy
and applicability of this method will only be enhanced by
extensive research using this method and in answering the
existing challenges and shortcomings.
REFERENCES
[1] G. Constantinides, F.-J.Ulm, K.VanVliet, "On the use of
nanoindentation for cementious materials" Materials and Structures,
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[2] Citing Websites.TheBrinell Hardness Test. Retrieved March 03,2013
from http://www.gordonengland.co.uklhardnesslbrinell.htm
[3] Citing WebsitesYickers Test. Retrieved March 03,2013 from
http://www.instron.us/wafapplications/test_types/hardness/vickers.aspx
thereby [4] Citing Websites.Rockwell indentation test principle. Retrieved March
03,2013 fromhttp://www.westportcorp.comlresourceslrockwell_hardnes
Uestl2.2.php
[5] F. Knoop, C.G. Peters and W.B. Emerson, "A Sensitive Pyramidal
Diamond Tool for Indentation Measurements", Journal of Research of
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[7] Giannakopoulos, A.E., Suresh. S, "Determination of elastoplastic
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[8] W. C. Oliver and G. M. Pharr, "An improved technique for
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[10] Y. T. Cheng and C. M. Cheng," Further analysis of indentation loading
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[12] Y. T. Cheng and C. M. Cheng," Can stress-strain relationships be
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[13] Y. T. Cheng and C. M. Cheng," General relationship between contact
stiifuess, contact depth and mechanical properties for indentation in
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linear viscoelastic solids using axisymmetric indenters of arbitrary

profiles", Applied Physics Letters, vol. 87(11), pp. 119-124, 2005.
[14] P. Mondal. "Nanomechanical Properties of Cementitious Materials",
Evanston, lllinois, 2008.
[15] S. Diamond and E. E. Lachowski, "On the morphology of type III C-S
H gel." Cement and Concrete Research, vol. 10, pp. 703-705, 1980.
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